新型键合纤维素手性固定相拆分氯西加酮对映体

目的: 建立一种用新型键合纤维素手性固定相拆分氯西加酮对映异构体的高效液相色谱方法。方法: 使用Chiralpak IB(250 mm×4.6 mm,5 μm)色谱柱,流动相为正己烷-无水乙醇(90︰10),流速0.8 mL·min^-1,检测波长230 nm,柱温30 ℃;通过对比氯西加酮和添加了苏式氯西加酮的氯西加酮色谱图,判断先流出物的构型。结果: 氯西加酮对映体在新型键合直链纤维素衍生化合物手性固定相上能够完全分离,分离度为1.79;先流出物为苏式氯西加酮。结论: 本方法可方便地实现氯西加酮对映体的分离。

Objective: To develop a liquid chromatographic method for the chiral separating enantiomers of losigamone. Methods: Losigamone enantiomers were separated by a Chiralpak IB(250 mm×4.6 mm,5 μm)at 30 ℃ and detected at 230 nm,the mobile phase used was n-hexane-ethanol(90:10)at a flow rate of 0.8 mL·min^-1.By comparing the chromatograph of enantiomers of losigamone and the chromatograph of losigamone spiked with threo-losigamone,determine the structure of the first effluent. Results: Losigamone enantiomers were separated on amylase derivative chiral stationary phase and the resolution was 1.79.The first effluent is threo-losigamone. Conclusion: The present method can be used for separating the enantiomers of losigamone simply.

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